JP6171851B2 - Apparatus row for seamless steel pipe production and method for producing high-strength stainless steel seamless steel pipe for oil wells using the same - Google Patents

Apparatus row for seamless steel pipe production and method for producing high-strength stainless steel seamless steel pipe for oil wells using the same Download PDF

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JP6171851B2
JP6171851B2 JP2013224235A JP2013224235A JP6171851B2 JP 6171851 B2 JP6171851 B2 JP 6171851B2 JP 2013224235 A JP2013224235 A JP 2013224235A JP 2013224235 A JP2013224235 A JP 2013224235A JP 6171851 B2 JP6171851 B2 JP 6171851B2
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steel pipe
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俊輔 佐々木
俊輔 佐々木
勝村 龍郎
龍郎 勝村
木村 秀途
秀途 木村
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JFE Steel Corp
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Priority to PCT/JP2014/004892 priority patent/WO2015064006A1/en
Priority to US15/032,421 priority patent/US10570471B2/en
Priority to RU2016121031A priority patent/RU2664582C2/en
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    • C21METALLURGY OF IRON
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    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B17/00Tube-rolling by rollers of which the axes are arranged essentially perpendicular to the axis of the work, e.g. "axial" tube-rolling
    • B21B17/08Tube-rolling by rollers of which the axes are arranged essentially perpendicular to the axis of the work, e.g. "axial" tube-rolling with mandrel having one or more protrusions, i.e. only the mandrel plugs contact the rolled tube; Press-piercing mills
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B19/00Tube-rolling by rollers arranged outside the work and having their axes not perpendicular to the axis of the work
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
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    • B21B19/02Tube-rolling by rollers arranged outside the work and having their axes not perpendicular to the axis of the work the axes of the rollers being arranged essentially diagonally to the axis of the work, e.g. "cross" tube-rolling ; Diescher mills, Stiefel disc piercers or Stiefel rotary piercers
    • B21B19/04Rolling basic material of solid, i.e. non-hollow, structure; Piercing, e.g. rotary piercing mills
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B23/00Tube-rolling not restricted to methods provided for in only one of groups B21B17/00, B21B19/00, B21B21/00, e.g. combined processes planetary tube rolling, auxiliary arrangements, e.g. lubricating, special tube blanks, continuous casting combined with tube rolling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
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    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
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    • C21D2211/008Martensite
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Description

本発明は、継目無鋼管の製造に係り、とくに継目無鋼管製造用として好適な装置列と、その装置列を利用した低温靭性に優れた油井用高強度ステンレス継目無鋼管の製造方法に関する。   The present invention relates to the production of seamless steel pipes, and more particularly to an apparatus row suitable for producing seamless steel pipes and a method for producing a high-strength stainless steel seamless pipe for oil wells having excellent low temperature toughness using the apparatus row.

近年、世界的なエネルギー消費量の増大による、原油等のエネルギー価格の高騰や、石油資源の枯渇という観点から、従来、省みられなかったような深度が深い油田(深層油田)や、硫化水素等を含む、いわゆるサワー環境下にある厳しい腐食環境の油田やガス田や、さらには厳しい気象環境の極北における油田やガス田等において、エネルギー資源開発が盛んに行われている。このような環境下で使用される油井用鋼管には、高強度で、かつ優れた耐食性(耐サワー性)や、さらには優れた低温靭性を兼ね備えた材質を有することが要求されている。   In recent years, from the viewpoint of soaring energy prices such as crude oil due to an increase in global energy consumption, and the depletion of petroleum resources, deep oil fields (deep oil fields) and hydrogen sulfide that have not been previously excluded Energy resources are being actively developed in oil fields and gas fields in severe corrosive environments under a so-called sour environment, and in oil fields and gas fields in the extreme north of severe weather environments. The oil well steel pipe used in such an environment is required to have a material having high strength and excellent corrosion resistance (sour resistance) and excellent low temperature toughness.

従来から、炭酸ガスCO、塩素イオンCl等を含む環境の油田、ガス田では、採掘に使用する油井管として13%Crマルテンサイト系ステンレス鋼管が多く使用されている。さらに、最近では13Crマルテンサイト系ステンレス鋼のCを低減し、Ni、Mo等を増加させた成分系の改良型13Crマルテンサイト系ステンレス鋼の使用も拡大している。
例えば、特許文献1には、13%Crマルテンサイト系ステンレス鋼の耐食性を改善した、改良型マルテンサイト系ステンレス鋼 (鋼板)の製造方法が記載されている。特許文献1に記載された技術では、重量%で10〜15%Crを含有するマルテンサイト系ステンレス鋼の組成で、Cを0.005〜0.05%と制限し、Ni:4.0%以上、Cu:0.5〜3%を複合添加し、さらにMoを1.0〜3%添加し、さらにNieqを−10以上に調整した組成を有する鋼を、熱間加工し室温まで自然放冷したのち、Ac1点以上でかつオーステナイト分率が80%になる温度以下で熱処理を施し、さらにオーステナイト分率が60%になる温度で熱処理を行い、組織が焼戻しマルテンサイト相、マルテンサイト相、残留オーステナイト相からなり、焼戻しマルテンサイト相、マルテンサイト相の合計の分率が60〜90%である組織を有する、マルテンサイトステンレス鋼としている。これにより、湿潤炭酸ガス環境および湿潤硫化水素環境における耐食性と耐硫化物応力腐食割れ性が向上するとしている。
Conventionally, 13% Cr martensitic stainless steel pipes are often used as oil well pipes used for mining in environmental oil fields and gas fields containing carbon dioxide CO 2 , chlorine ions Cl − and the like. Furthermore, recently, the use of improved 13Cr martensitic stainless steels with a reduced content of 13Cr martensitic stainless steel and increased Ni, Mo, etc. has been expanded.
For example, Patent Document 1 describes a method for producing an improved martensitic stainless steel (steel plate) in which the corrosion resistance of 13% Cr martensitic stainless steel is improved. In the technique described in Patent Document 1, the composition of martensitic stainless steel containing 10 to 15% Cr by weight is limited to 0.005 to 0.05% for C, Ni: 4.0% or more, Cu: 0.5 to A steel with a composition with 3% added, Mo added 1.0 to 3% and Nieq adjusted to -10 or higher is hot-worked and allowed to cool naturally to room temperature. Heat treatment is performed below the temperature at which the fraction reaches 80%, heat treatment is performed at a temperature at which the austenite fraction reaches 60%, and the structure is composed of a tempered martensite phase, a martensite phase, and a retained austenite phase. The martensitic stainless steel has a structure in which the total fraction of the martensite phase is 60 to 90%. As a result, the corrosion resistance and sulfide stress corrosion cracking resistance in a wet carbon dioxide environment and a wet hydrogen sulfide environment are improved.

また、特許文献2には、耐食性に優れた油井用高強度ステンレス鋼管の製造方法が記載されている。特許文献2に記載された技術では、mass%で、C:0.005〜0.050%、Si:0.05〜0.50%、Mn:0.20〜1.80%、Cr:15.5〜18%、Ni:1.5〜5%、Mo:1〜3.5%、V:0.02〜0.20%、N:0.01〜0.15%、O:0.006%以下を含有し、Cr+0.65Ni+0.6Mo+0.55Cu−20C≧19.5およびCr+Mo+0.3Si−43.5C−0.4Mn−Ni−0.3Cu−9N≧11.5を満足する組成を有する鋼管素材を加熱し、熱間加工により造管して、造管後、空冷以上の冷却速度で室温まで冷却して所定寸法の継目無鋼管とし、ついで継目無鋼管を、850℃以上の温度に再加熱し空冷以上の冷却速度で100℃以下まで冷却し、ついで700℃以下の温度に加熱する焼入れ−焼戻処理を施すことにより、体積率で10〜60%のフェライト相を含み残部がマルテンサイト相である組織を有し、降伏強さが654MPa以上の油井用高強度ステンレス鋼管を得ることができるとしている。これにより、高強度で、COやClを含む、230℃までの高温の厳しい腐食環境下においても充分な耐食性を有し、しかもシャルピー衝撃試験の−40℃での吸収エネルギーが50J以上の高靭性を有する鋼管となるとしている。 Patent Document 2 describes a method for producing a high-strength stainless steel pipe for oil wells having excellent corrosion resistance. In the technique described in Patent Document 2, in mass%, C: 0.005 to 0.050%, Si: 0.05 to 0.50%, Mn: 0.20 to 1.80%, Cr: 15.5 to 18%, Ni: 1.5 to 5%, Mo : 1 to 3.5%, V: 0.02 to 0.20%, N: 0.01 to 0.15%, O: 0.006% or less, Cr + 0.65Ni + 0.6Mo + 0.55Cu-20C ≧ 19.5 and Cr + Mo + 0.3Si-43.5C-0.4Mn -Ni-0.3Cu-9N≥11.5 steel pipe material is heated, piped by hot working, and then piped and then cooled to room temperature at a cooling rate equal to or higher than that of air cooling to seamlessly pass through the specified dimensions. By performing a quenching-tempering treatment in which the steel pipe is then reheated to a temperature of 850 ° C or higher, cooled to 100 ° C or lower at a cooling rate of air cooling or higher, and then heated to a temperature of 700 ° C or lower. A high-strength stainless steel pipe for oil wells having a structure containing a ferrite phase of 10 to 60% by volume and the balance being a martensite phase and a yield strength of 654 MPa or more can be obtained. To have. Accordingly, high strength, CO 2 and Cl - containing, has sufficient corrosion resistance even at a high temperature severe corrosive environments up to 230 ° C., moreover absorbed energy at -40 ℃ Charpy impact test is more than 50J The steel pipe has high toughness.

特開平10−1755号公報Japanese Patent Laid-Open No. 10-1755 特許第5109222号公報Japanese Patent No. 5109222

油井用継目無鋼管には、種々の肉厚、径の鋼管が要求される。とくに、厚肉継目無鋼管の製造においては、肉厚が厚くなるにしたがい、通常の熱間加工法では、加工歪を肉厚中心までに付与することが難しくなり、肉厚中心部の組織が粗大化する傾向となる。そのため、薄肉鋼管に比べて厚肉鋼管では、肉厚中央部の靭性が低下しやすい。特許文献1,2に記載された技術では、高々肉厚12.7mmまでの鋼管を対象としており、特許文献1,2には、それ以上の厚肉継目無鋼管の低温靭性向上についてまでの言及はない。   Steel pipes of various thicknesses and diameters are required for oil well seamless steel pipes. In particular, in the manufacture of thick-walled seamless steel pipes, as the wall thickness increases, the normal hot working method makes it difficult to apply processing strain to the center of the wall thickness, and the structure of the wall thickness center part becomes difficult. It tends to be coarse. Therefore, compared with a thin steel pipe, in a thick steel pipe, the toughness of the thickness center part tends to decrease. The techniques described in Patent Documents 1 and 2 are intended for steel pipes with a thickness of up to 12.7 mm, and Patent Documents 1 and 2 refer to the improvement in low-temperature toughness of thick-walled seamless steel pipes. Absent.

かかる従来技術の状況に鑑み、本発明は、優れた低温靭性を有する厚肉ステンレス継目無鋼管を安価に製造できる、継目無鋼管製造用装置列を提供することを目的とする。また、本発明は、それら装置列を利用して、降伏強さ:654MPaを超える高強度と、高温腐食環境下での優れた耐食性と、肉厚中心部での優れた低温靭性とを兼備する油井用高強度厚肉ステンレス継目無鋼管を得ることができる、油井用高強度厚肉ステンレス継目無鋼管の製造方法を提供することを目的とする。なお、ここでいう「厚肉継目無鋼管」とは、肉厚13mm超え100mm程度以下の継目無鋼管をいうものとする。   In view of the state of the prior art, it is an object of the present invention to provide a device array for manufacturing seamless steel pipes that can inexpensively manufacture a thick stainless steel seamless steel pipe having excellent low temperature toughness. In addition, the present invention combines these devices with high strength exceeding yield strength: 654 MPa, excellent corrosion resistance under a high temperature corrosion environment, and excellent low temperature toughness at the center of the thickness. It is an object of the present invention to provide a method for producing a high-strength thick stainless steel seamless steel pipe for oil wells, which can provide a high-strength thick stainless steel seamless steel pipe for oil wells. The term “thick-walled seamless steel pipe” as used herein refers to a seamless steel pipe having a wall thickness exceeding 13 mm and not more than about 100 mm.

本発明者らは、上記した目的を達成するために、厚肉ステンレス継目無鋼管肉厚中央部の靭性に及ぼす各種要因について鋭意研究した。その結果、靭性改善に最も有効な方法は、組織の微細化であるということに思い至った。
そこで、更なる研究を行ない、厚肉マルテンサイト系ステンレス継目無鋼管の組織微細化のためには、穿孔圧延後の中空素材に、600℃以上の温度域で、少なくとも50℃以上の温度範囲を、空冷以上の冷却速度である1.0℃/s以上の平均冷却速度で冷却を施し、さらに減肉あるいは成形等の加工を施せば、組織が微細化し、肉厚:13mmを超える厚肉ステンレス継目無鋼管の肉厚中心位置においても低温靭性が顕著に向上するという知見を得た。
In order to achieve the above-mentioned object, the present inventors diligently studied various factors affecting the toughness of the thick-walled stainless steel seamless steel tube wall thickness central portion. As a result, it came to mind that the most effective method for improving toughness is the refinement of the structure.
In order to refine the structure of the thick-walled martensitic stainless steel seamless tube, the hollow material after piercing and rolling should have a temperature range of 600 ° C or higher and a temperature range of 50 ° C or higher. Cooling at an average cooling rate of 1.0 ° C / s or higher, which is a cooling rate higher than air cooling, and further reducing the thickness or processing such as forming, the structure becomes finer and the wall thickness: 13 mm thick stainless steel seamless The knowledge that low temperature toughness is remarkably improved also at the thickness center position of the steel pipe was obtained.

まず、本発明者らが行った本発明の基礎となった実験結果について説明する。
質量%で、0.017%C−0.19%Si−0.26%Mn−0.01%P−0.002%S−16.6%Cr−3.5%Ni−1.6%Mo−0.047%V−0.047%N−0.01%Al−残部Feからなる組成の油井用マルテンサイト系ステンレス継目無鋼管から試験材を採取した。採取した試験材を、加熱温度:1250℃に加熱し一定時間(60min)保持したのち、熱間加工温度範囲である1200〜600℃の範囲の冷却停止温度までを種々の冷却速度で冷却した。冷却終了後、試験材を直ちに急冷して、組織を凍結した。
First, the experimental results that were the basis of the present invention conducted by the present inventors will be described.
0.017% C-0.19% Si-0.26% Mn-0.01% P-0.002% S-16.6% Cr-3.5% Ni-1.6% Mo-0.047% V-0.047% N-0.01% Al-balance Fe A test material was collected from a martensitic stainless steel seamless pipe for an oil well having a composition consisting of: The collected test material was heated to a heating temperature of 1250 ° C. and held for a certain time (60 min), and then cooled at various cooling rates up to a cooling stop temperature in the range of 1200 to 600 ° C. which is a hot working temperature range. After completion of cooling, the test material was immediately quenched to freeze the tissue.

ついで、得られた試験片を研磨、腐食(腐食液:ビレラ液)して組織を観察し、マルテンサイト相とフェライト相の面積率を測定した。なお、マルテンサイト相は、冷却停止温度で存在したオーステナイト相が急冷時に変態したものである。得られた結果を、平均冷却速度と冷却停止温度でのフェライト量(面積率)との関係で、図2に示す。
図2から、冷却停止温度によらず、加熱温度から冷却停止温度(熱間加工温度)までの温度範囲を、1.0℃/s以上の平均冷却速度で冷却することにより、0.5℃/sで冷却した場合よりも、フェライト相分率が多くなることがわかる。なお、平均冷却速度:0.5℃/sの冷却は、空冷を模擬した冷却(空冷相当)であり、平衡に近い状態での冷却であるといえる。
Subsequently, the obtained test piece was polished and corroded (corrosion solution: Villera solution), and the structure was observed, and the area ratios of the martensite phase and the ferrite phase were measured. The martensite phase is a phase in which the austenite phase present at the cooling stop temperature is transformed upon rapid cooling. The obtained results are shown in FIG. 2 in relation to the average cooling rate and the ferrite amount (area ratio) at the cooling stop temperature.
From FIG. 2, regardless of the cooling stop temperature, the temperature range from the heating temperature to the cooling stop temperature (hot working temperature) is cooled at 0.5 ° C./s by cooling at an average cooling rate of 1.0 ° C./s or more. It can be seen that the ferrite phase fraction is higher than that of the case. The cooling at an average cooling rate of 0.5 ° C./s is a cooling simulating air cooling (equivalent to air cooling) and can be said to be cooling in a state close to equilibrium.

すなわち、上記したような組成のマルテンサイト系ステンレス鋼においては、通常、加熱温度域では、フェライト相の分率が高く、加熱温度から空冷程度の冷却速度で冷却すると、温度の低下に伴い、フェライト相が減少してオーステナイト相の分率が増加する。しかし、加熱温度から熱間加工温度(冷却停止温度)までの温度範囲を、1.0℃/s以上の平均冷却速度で加速冷却することにより、オーステナイト相の析出が遅れ、フェライト相が平衡状態より多く残存して、非平衡状態の相分布(組織)が得られる。   That is, in the martensitic stainless steel having the composition described above, the ferrite phase fraction is usually high in the heating temperature range, and when cooling from the heating temperature to a cooling rate of about air cooling, the ferrite decreases with decreasing temperature. The phase decreases and the fraction of the austenite phase increases. However, accelerated cooling of the temperature range from the heating temperature to the hot working temperature (cooling stop temperature) at an average cooling rate of 1.0 ° C / s or more delays the precipitation of the austenite phase and increases the ferrite phase from the equilibrium state. It remains and a non-equilibrium phase distribution (structure) is obtained.

そして、本発明者らは、このような非平衡状態の組織となった材料に、加工(圧延)を施せば、組織の微細化が達成できることを見い出した。というのは、非平衡で存在するフェライト粒に歪を付加すれば、α→γ変態の核生成サイトが多数生成でき、その結果、変態後に生成するオーステナイト粒が微細化し、低温靭性が向上すると考えられる。
そして、本発明者らは、上記した現象を利用して低温靭性に優れた油井用ステンレス継目無鋼管を製造可能とするためには、使用する装置列を、加熱装置と穿孔圧延装置と圧延装置とをこの順に配列した従来の装置列から、加熱装置と穿孔圧延装置の間、あるいは穿孔圧延装置と圧延装置の間に、冷却装置を配設した装置列とすることが肝要であることを知見した。
The present inventors have found that the structure can be made finer by subjecting the material having such a non-equilibrium structure to processing (rolling). This is because, if strain is added to the ferrite grains that exist in non-equilibrium, a large number of α → γ transformation nucleation sites can be generated, and as a result, the austenite grains generated after the transformation become finer and the low temperature toughness is improved. It is done.
And in order to make it possible to produce a stainless steel seamless steel pipe for oil wells having excellent low-temperature toughness using the above-mentioned phenomenon, the present inventors have used a device row, a heating device, a piercing and rolling device, and a rolling device. It is found that it is important to use a device row in which a cooling device is arranged between the heating device and the piercing and rolling device or between the piercing and rolling device and the rolling device, from the conventional device row in which the above are arranged in this order. did.

本発明は、かかる知見に基づき、更なる検討を加えて完成されたものである。すなわち、本発明の要旨はつぎの通りである。
(1)鋼素材を加熱する加熱装置と、該加熱された鋼素材に穿孔圧延を施し中空素材とする穿孔圧延装置と、該中空素材に加工を施し所定形状の継目無鋼管とする圧延装置とをこの順に配設してなる継目無鋼管製造用装置列において、前記加熱装置と前記穿孔圧延装置との間に、または前記穿孔圧延装置と前記圧延装置との間に、被冷却材の外表面位置の平均冷却速度で1.0℃/s以上の冷却能を有する冷却装置を配設してなることを特徴とする厚肉ステンレス継目無鋼管製造用装置列。
The present invention has been completed on the basis of such findings and further studies. That is, the gist of the present invention is as follows.
(1) A heating device for heating a steel material, a piercing and rolling device for subjecting the heated steel material to piercing and rolling to form a hollow material, and a rolling device for processing the hollow material to obtain a seamless steel pipe having a predetermined shape. Are arranged in this order, in an apparatus row for seamless steel pipe production, between the heating device and the piercing-rolling device or between the piercing-rolling device and the rolling device, the outer surface of the material to be cooled An apparatus row for manufacturing a thick-walled stainless steel seamless pipe comprising a cooling apparatus having a cooling capacity of 1.0 ° C./s or more at an average cooling rate at a position .

(2)(1)において、前記圧延装置の出側に、保温装置を配設することを特徴とする厚肉ステンレス継目無鋼管製造用装置列。
)(1)または(2)に記載の厚肉ステンレス継目無鋼管製造用装置列を利用した厚肉ステンレス継目無鋼管の製造方法であって、鋼素材を前記加熱装置で加熱後、前記穿孔圧延装置で穿孔圧延を施して中空素材とし、さらに該中空素材を前記冷却装置で冷却したのち、前記圧延装置で加工を施して、あるいはさらに該加工後に前記保温装置を通過させる処理を施して、さらに焼入焼戻処理あるいは焼戻処理からなる熱処理を施し、所定寸法の厚肉ステンレス継目無鋼管とするにあたり、前記鋼素材を、質量%で、C:0.050%以下、Si:0.50%以下、Mn:0.20〜1.80%、Cr:15.5〜18.0%、Ni:1.5〜5.0%、Mo:1.0〜3.5%、V:0.02〜0.20%、N:0.01〜0.15%、O:0.006%以下を含み、残部Feおよび不可避的不純物からなる組成を有する鋼素材とし、前記加熱を、600℃以上鋼素材の融点未満の温度に加熱する処理とし、前記穿孔圧延を施したのちで、前記冷却装置で冷却する前の前記中空素材の表面温度を冷却開始温度として、前記冷却を、表面温度で、前記冷却開始温度からの温度差が少なくとも50℃以上で、かつ600℃以上となる冷却停止温度まで、外表面温度で1.0℃/s以上の平均冷却速度で冷却する処理とし、前記厚肉ステンレス継目無鋼管が、管軸方向の降伏強さが654MPa超えの高強度と、肉厚中心部でシャルピー衝撃試験の試験温度:−40℃での管軸方向における吸収エネルギーが50J以上となる優れた低温靭性とを兼備する高強度厚肉ステンレス継目無鋼管であることを特徴とする低温靭性に優れた油井用高強度厚肉ステンレス継目無鋼管の製造方法。
(2) Oite to (1), the delivery side of the rolling apparatus, the thick stainless seamless steel manufacturing equipment train, characterized by disposing the heat insulating device.
(3) (1) or (2) a method of manufacturing a thick-walled stainless seamless steel pipe using a thick stainless seamless steel manufacturing equipment train according, after heating the steel material in the heating device, wherein A hollow material is formed by piercing and rolling with a piercing and rolling device, and the hollow material is further cooled with the cooling device, then processed with the rolling device, or further subjected to a process of passing through the heat retaining device after the processing. Furthermore, when a heat treatment consisting of quenching and tempering treatment or tempering treatment is performed to make a thick stainless steel seamless steel pipe of a predetermined size, the steel material is in mass%, C: 0.050% or less, Si: 0.50% or less , Mn: 0.20-1.80%, Cr: 15.5-18.0%, Ni: 1.5-5.0%, Mo: 1.0-3.5%, V: 0.02-0.20%, N: 0.01-0.15%, O: 0.006% or less A steel material having a composition comprising the balance Fe and inevitable impurities, and the heating In addition, the heat treatment is performed at a temperature of 600 ° C. or higher and less than the melting point of the steel material, and after the piercing and rolling, the surface temperature of the hollow material before cooling with the cooling device is set as a cooling start temperature, and the cooling is performed. At the surface temperature, the temperature difference from the cooling start temperature is at least 50 ° C. or more, and the cooling is performed at an average cooling rate of 1.0 ° C./s or more at the outer surface temperature to the cooling stop temperature at which the temperature is 600 ° C. or more . The above-mentioned thick stainless steel seamless steel pipe has a high strength with a yield strength exceeding 654 MPa in the tube axis direction, and a Charpy impact test temperature at the center of the wall thickness: absorbed energy in the tube axis direction at −40 ° C. is 50 J or more A method for producing a high-strength thick stainless steel seamless steel pipe for oil wells having excellent low-temperature toughness, characterized by being a high-strength thick-walled stainless steel seamless steel pipe having both excellent low-temperature toughness.

)()において、前記加工後に前記保温装置内を通過させる処理が、平均冷却速度で20℃/s以下の冷却となるように調整する処理とすることを特徴とする油井用高強度厚肉ステンレス継目無鋼管の製造方法。
)()または()において、前記組成に加えてさらに、質量%で、次A群〜D群
A群:Al:0.002〜0.050%、
B群:Cu:3.5%以下、
C群:Nb:0.2%以下、Ti:0.3%以下、Zr:0.2%以下、W:3.0%以下、B:0.01%以下のうちから選ばれた1種または2種以上、
D群:Ca:0.01%以下、REM:0.01%以下のうちから選ばれた1種または2種
のうちから選ばれた1群または2群以上を含有することを特徴とする油井用高強度ステンレス継目無鋼管の製造方法。
( 4 ) In ( 3 ), the process of passing through the heat retaining device after the processing is a process of adjusting the cooling so that the average cooling rate is 20 ° C./s or less. Manufacturing method for thick-walled stainless steel seamless steel pipe.
( 5 ) In ( 3 ) or ( 4 ), in addition to the above-mentioned composition, the following groups A to D: Group A: Al: 0.002 to 0.050%
Group B: Cu: 3.5% or less,
Group C: Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less, W: 3.0% or less, B: 0.01% or less selected from 0.01% or less,
D group: Ca: 0.01% or less, REM: High strength stainless steel for oil wells containing one or more groups selected from one or two selected from 0.01% or less A method for producing seamless steel pipes.

本発明によれば、低温靭性に優れた厚肉高強度ステンレス継目無鋼管を、容易に製造でき、産業上格段の効果を奏する。また、本発明によれば、比較的少ない加工量で鋼管組織を中心部まで微細化することができ、肉厚中心位置での加工量を大きくすることができない厚肉継目無鋼管でも、低温靭性の向上が図れるという効果がある。   According to the present invention, a thick high-strength stainless steel seamless pipe excellent in low-temperature toughness can be easily manufactured, and an industrially remarkable effect is achieved. In addition, according to the present invention, the steel pipe structure can be refined to the center with a relatively small amount of processing, and even in thick-walled seamless steel pipes where the amount of processing at the center of the wall thickness cannot be increased, There is an effect that the improvement can be achieved.

本発明継目無鋼管製造用装置列の一例を模式的に示す説明図である。It is explanatory drawing which shows typically an example of the apparatus row | line | column for this invention seamless steel pipe manufacture. 熱間加工前の平均冷却速度と冷却停止温度でのフェライト量との関係を示すグラフである。It is a graph which shows the relationship between the average cooling rate before hot processing, and the ferrite content in cooling stop temperature.

本発明継目無鋼管製造用装置列は、加熱した鋼素材を適正温度範囲内で冷却したのちに、加工を施し、継目無鋼管とすることができる装置列とする。本発明継目無鋼管製造用装置列の一例を図1に示す。本発明継目無鋼管製造用装置列は、(a)加熱装置1と穿孔圧延装置2と冷却装置4と圧延装置3とをこの順に配設、あるいは(b)加熱装置1と冷却装置4と穿孔圧延装置2と圧延装置3とをこの順に配設、してなる装置列とする。   The apparatus row for manufacturing the seamless steel pipe of the present invention is an apparatus row that can be processed into a seamless steel pipe after cooling the heated steel material within an appropriate temperature range. An example of the apparatus row | line | column for this invention seamless steel pipe manufacture is shown in FIG. The apparatus row | line | column for this invention seamless steel pipe manufacture arrange | positions the heating apparatus 1, the piercing-rolling apparatus 2, the cooling apparatus 4, and the rolling apparatus 3 in this order, or (b) the heating apparatus 1, the cooling apparatus 4, and piercing | punching. The rolling device 2 and the rolling device 3 are arranged in this order to form a device row.

本発明で使用する加熱装置1は、丸鋳片、丸鋼片等の鋼素材を所定温度に加熱できる、例えば、回転炉床式加熱炉、ウォーキングビーム式加熱炉等の常用の加熱炉がいずれも適用できる。また、誘導加熱方式の加熱炉としてもよい。
また、本発明で使用する穿孔圧延装置2は、加熱された鋼素材に穿孔圧延を施し中空素材とすることができる穿孔圧延装置であればよく、例えば、バレル形ロール等を用いるマンネスマン傾斜式穿孔機、熱間押出式穿孔機等の、通常公知の穿孔圧延装置がいずれも適用できる。
The heating apparatus 1 used in the present invention can heat steel materials such as round cast pieces and round steel pieces to a predetermined temperature. For example, a conventional heating furnace such as a rotary hearth type heating furnace or a walking beam type heating furnace can be used. Is also applicable. Alternatively, an induction heating type heating furnace may be used.
Further, the piercing and rolling apparatus 2 used in the present invention may be any piercing and rolling apparatus that can perform piercing and rolling on a heated steel material to form a hollow material. For example, Mannesmann inclined piercing using a barrel-shaped roll or the like. Any generally known piercing and rolling apparatus such as a machine or a hot extrusion piercing machine can be applied.

また、本発明で使用する圧延装置3は、中空素材に加工を施し所定形状の継目無鋼管とすることができる装置であればよく、目的に応じて、例えば、エロンゲータ31、穿孔された中空素管を薄く長く延ばすプラグミル32、素管内外表面を滑らかにするリーラ(図示せず)、所定寸法に整えるサイザー33の順で配置された圧延装置、あるいは中空素管を所定寸法の鋼管とするマンドレルミル(図示せず)、若干の圧下を行ない外径、肉厚を調整するレデューサ(図示せず)を配置した圧延装置等の、通常公知の圧延装置がいずれも適用できる。なお、好ましくは加工量を大きくとれるエロンゲータ、あるいはマンドレルミルとすることが好ましい。   The rolling device 3 used in the present invention may be any device that can process a hollow material into a seamless steel pipe having a predetermined shape. For example, an elongator 31 or a perforated hollow element can be used depending on the purpose. A rolling mill arranged in the order of a plug mill 32 for extending the tube thinly and long, a reeler (not shown) for smoothing the inner and outer surfaces of the tube, a sizer 33 for adjusting the tube to a predetermined size, or a mandrel having a hollow tube as a steel tube of a predetermined size Any generally known rolling device such as a mill (not shown), a rolling device provided with a reducer (not shown) that slightly reduces the outer diameter and adjusts the wall thickness can be applied. In addition, it is preferable to use an elongator or mandrel mill that can take a large amount of processing.

また、本発明で使用する冷却装置4は、非平衡状態の相分布を得るために、加熱装置1と穿孔圧延装置2の間、あるいは穿孔圧延装置2と圧延装置3との間に設置される。本発明で使用する冷却装置は、加熱された鋼素材(被冷却材)を所望の冷却速度以上で冷却することが可能な装置であれば、その形式はとくに限定する必要はない。比較的容易に所望の冷却速度を確保できる冷却装置としては、被冷却材である加熱された鋼素材あるいは中空素材の外内面に、冷却水または圧縮空気、ミストを噴射して、あるいは供給して冷却する方式の装置とすることが好ましい。   The cooling device 4 used in the present invention is installed between the heating device 1 and the piercing and rolling device 2 or between the piercing and rolling device 2 and the rolling device 3 in order to obtain a non-equilibrium phase distribution. . The type of the cooling device used in the present invention is not particularly limited as long as it is a device capable of cooling a heated steel material (cooled material) at a desired cooling rate or higher. As a cooling device that can secure a desired cooling rate relatively easily, cooling water, compressed air, or mist is injected or supplied to the outer surface of a heated steel material or hollow material that is a material to be cooled. It is preferable to use a cooling system.

本発明で使用する冷却装置は、ステンレス鋼組成の鋼管製造に際しては、非平衡状態の相分布を得るために、被冷却材の外表面位置で、少なくとも1.0℃/s以上の平均冷却速度を得ることができる冷却能を有する装置とする必要がある。冷却装置の冷却能が不足し、上記した平均冷却速度より遅い冷却しかできない場合には、非平衡状態の相分布を得ることができず、その後に加工を施しても、組織の微細化ができなくなる。なお、冷却速度の上限は、とくに限定する必要はないが、熱応力による割れや曲がりの防止という観点から、30℃/sとすることが好ましい。   The cooling device used in the present invention obtains an average cooling rate of at least 1.0 ° C./s or more at the outer surface position of the material to be cooled in order to obtain a non-equilibrium phase distribution when manufacturing a steel pipe having a stainless steel composition. It is necessary to provide a device having a cooling capacity that can be used. If the cooling capacity of the cooling device is insufficient and cooling can only be performed slower than the average cooling rate described above, a phase distribution in a non-equilibrium state cannot be obtained, and the microstructure can be refined even after subsequent processing. Disappear. The upper limit of the cooling rate is not particularly limited, but is preferably 30 ° C./s from the viewpoint of preventing cracking and bending due to thermal stress.

なお、本発明では、圧延装置3の出側に、保温装置(図示せず)を配設した装置列とすることが好ましい。本発明では、圧延加工後の冷却速度を遅くするために、保温装置を配設する。ステンレス鋼管の場合、加工後に冷却が速すぎると、非平衡フェライト相がα→γ変態を生じることなく冷却され、微細なオーステナイト粒の生成が得られず、所望の鋼管組織の微細化が達成できなくなる。なお、保温装置は、被冷却材の表面位置で、少なくとも20℃/s以下程度の冷却速度に調整できる保温能があれば十分である。   In the present invention, it is preferable to use a device row in which a heat retaining device (not shown) is provided on the exit side of the rolling device 3. In this invention, in order to slow down the cooling rate after a rolling process, a heat retention apparatus is arrange | positioned. In the case of stainless steel pipe, if the cooling is too fast after processing, the nonequilibrium ferrite phase is cooled without causing the α → γ transformation, and fine austenite grains cannot be formed, and the desired refinement of the steel pipe structure can be achieved. Disappear. Note that it is sufficient for the heat retaining device to have a heat retaining ability that can be adjusted to a cooling rate of at least about 20 ° C./s at the surface position of the material to be cooled.

つぎに、上記した本発明継目無鋼管製造用装置列を利用して、高強度で、耐食性に優れ、かつ低温靭性に優れた油井用厚肉高強度ステンレス継目無鋼管の製造方法について説明する。
鋼素材を前記加熱装置で加熱したのち、穿孔圧延装置で穿孔圧延を施して中空素材とし、さらに中空素材を冷却装置で冷却したのち、直ちに圧延装置で加工を施して、あるいは加工後にさらに保温装置を通過させる処理を施し、所定寸法の継目無鋼管とする。
Next, a method for producing a thick high-strength stainless steel seamless steel pipe for oil wells that is high in strength, excellent in corrosion resistance, and excellent in low-temperature toughness will be described using the above-described apparatus for producing a seamless steel pipe of the present invention.
After the steel material is heated by the heating device, the steel material is pierced and rolled by a piercing and rolling device to form a hollow material, and the hollow material is further cooled by a cooling device, and then immediately processed by the rolling device, or after the processing, a further heat retaining device. To give a seamless steel pipe of a predetermined size.

使用する鋼素材は、質量%で、C:0.050%以下、Si:0.50%以下、Mn:0.20〜1.80%、Cr:15.5〜18.0%、Ni:1.5〜5.0%、Mo:1.0〜3.5%、V:0.02〜0.20%、N:0.01〜0.15%、O:0.006%以下を含み、残部Feおよび不可避的不純物からなる組成を有する。
まず、鋼素材の組成の限定理由について説明する。なお、とくに断わらないかぎり、質量%は単に%で記す。
The steel materials used are mass%, C: 0.050% or less, Si: 0.50% or less, Mn: 0.20 to 1.80%, Cr: 15.5 to 18.0%, Ni: 1.5 to 5.0%, Mo: 1.0 to 3.5%, V: 0.02 to 0.20%, N: 0.01 to 0.15%, O: 0.006% or less, and a composition comprising the balance Fe and inevitable impurities.
First, the reasons for limiting the composition of the steel material will be described. Unless otherwise specified, mass% is simply expressed as%.

C:0.050%以下
Cは、マルテンサイト系ステンレス鋼の強度に関係する重要な元素であり、本発明では所望の強度を確保するために0.005%以上含有することが望ましい。一方、0.050%を超えて含有すると、Ni含有による焼戻時の鋭敏化が増大する。なお、耐食性の観点からはCは少ないほうが望ましい。このようなことから、Cは0.050%以下に限定した。なお、好ましくは0.030〜0.050%である。
C: 0.050% or less
C is an important element related to the strength of martensitic stainless steel. In the present invention, C is preferably contained in an amount of 0.005% or more in order to ensure a desired strength. On the other hand, if the content exceeds 0.050%, sensitization during tempering due to Ni inclusion increases. From the viewpoint of corrosion resistance, it is desirable that C is small. For these reasons, C is limited to 0.050% or less. In addition, Preferably it is 0.030 to 0.050%.

Si:0.50%以下
Siは、脱酸剤として作用する元素であり、0.05%以上含有することが望ましい。一方、0.50%を超える含有は、耐食性を低下させ、さらに熱間加工性をも低下させる。このため、Siは0.50%以下に限定した。なお、好ましくは0.10〜0.30%である。
Mn:0.20〜1.80%
Mnは、強度を増加させる作用を有する元素であり、このような効果を得るためには0.20%以上の含有を必要とする。一方、1.80%を超えて含有すると、靭性に悪影響を及ぼす。このため、Mnは0.20〜1.80%に限定した。なお、好ましくは0.2〜1.0%である。
Si: 0.50% or less
Si is an element that acts as a deoxidizer, and it is desirable to contain 0.05% or more. On the other hand, if the content exceeds 0.50%, the corrosion resistance is lowered and the hot workability is also lowered. For this reason, Si was limited to 0.50% or less. In addition, Preferably it is 0.10 to 0.30%.
Mn: 0.20 to 1.80%
Mn is an element having an action of increasing the strength, and in order to obtain such an effect, it needs to be contained in an amount of 0.20% or more. On the other hand, if the content exceeds 1.80%, the toughness is adversely affected. For this reason, Mn was limited to 0.20 to 1.80%. In addition, Preferably it is 0.2 to 1.0%.

Cr:15.5〜18.0%
Crは、保護皮膜を形成し耐食性を向上させる作用を有し、さらに固溶して鋼の強度を増加させる元素である。このような効果を得るためには、15.5%以上の含有を必要とする。一方、18.0%を超えて多量に含有すると、熱間加工性が低下し、さらに強度が低下する。このため、Crは15.5〜18.0%に限定した。なお、好ましくは16.5〜18.0%である。
Cr: 15.5-18.0%
Cr is an element that has a function of forming a protective film and improving the corrosion resistance, and further increasing the strength of the steel by solid solution. In order to obtain such an effect, the content of 15.5% or more is required. On the other hand, if the content exceeds 18.0%, the hot workability is lowered and the strength is further lowered. For this reason, Cr was limited to 15.5-18.0%. In addition, Preferably it is 16.5-18.0%.

Ni:1.5〜5.0%
Niは、保護膜を強固にし、耐食性を高める作用を有する元素であり、さらに固溶して鋼の強度を増加させ、さらに靭性を向上させる元素でもある。このような効果は1.5%以上の含有で認められる。一方、5.0%を超えて含有すると、マルテンサイト相の安定性が低下し、強度が低下する。このため、Niは1.5〜5.0%に限定した。なお、好ましくは2.5〜4.5%である。
Ni: 1.5-5.0%
Ni is an element that has an action of strengthening the protective film and improving the corrosion resistance, and further increasing the strength of the steel by solid solution and further improving the toughness. Such an effect is recognized when the content is 1.5% or more. On the other hand, if the content exceeds 5.0%, the stability of the martensite phase decreases and the strength decreases. For this reason, Ni was limited to 1.5 to 5.0%. In addition, Preferably it is 2.5 to 4.5%.

Mo:1.0〜3.5%
Moは、Clによる孔食に対する抵抗性を増加させる元素であり、1.0%以上の含有を必要とする。一方、3.5%を超える多量の含有は、強度が低下するとともに、材料コストが高騰する。このため、Moは1.0〜3.5%に限定した。なお、好ましくは2〜3.5%である。
V:0.02〜0.20%
Vは、強度を増加させるとともに、耐食性を改善する元素である。このような効果を得るためには、0.02%以上の含有を必要とする。一方、0.20%を超えて含有すると、靭性が低下する。このため、Vは0.02〜0.20%に限定した。なお、好ましくは0.02〜0.08%である。
Mo: 1.0-3.5%
Mo is an element that increases resistance to pitting corrosion caused by Cl , and needs to be contained in an amount of 1.0% or more. On the other hand, if the content exceeds 3.5%, the strength decreases and the material cost increases. For this reason, Mo was limited to 1.0 to 3.5%. In addition, Preferably it is 2 to 3.5%.
V: 0.02 to 0.20%
V is an element that increases strength and improves corrosion resistance. In order to obtain such an effect, a content of 0.02% or more is required. On the other hand, if the content exceeds 0.20%, toughness decreases. For this reason, V was limited to 0.02 to 0.20%. In addition, Preferably it is 0.02 to 0.08%.

N:0.01〜0.15%
Nは、耐孔食性を著しく向上される元素であり、このような効果を得るためには0.01%以上の含有を必要とする。一方、0.15%を超えて含有すると、種々の窒化物を形成し靭性を低下させる。なお、好ましくは0.02〜0.08%である。
O:0.006%以下
Oは、鋼中では酸化物として存在し、各種特性に悪影響を及ぼす。このため、できるだけ低減することが望ましい。とくに、Oが0.006%を超えて多量に含有すると、熱間加工性、靭性、耐食性の低下が著しくなる。このため、Oは0.006%以下に限定した。
N: 0.01-0.15%
N is an element that remarkably improves the pitting corrosion resistance. In order to obtain such an effect, N is required to be contained in an amount of 0.01% or more. On the other hand, if the content exceeds 0.15%, various nitrides are formed and the toughness is lowered. In addition, Preferably it is 0.02 to 0.08%.
O: 0.006% or less
O exists as an oxide in steel and adversely affects various properties. For this reason, it is desirable to reduce as much as possible. In particular, when O is contained in a large amount exceeding 0.006%, the hot workability, toughness and corrosion resistance are remarkably deteriorated. For this reason, O was limited to 0.006% or less.

上記した成分が基本の成分であるが、基本成分に加えてさらに、選択元素として、次A群〜D群
A群:Al:0.002〜0.050%、
B群:Cu:3.5%以下、
C群:Nb:0.2%以下、Ti:0.3%以下、Zr:0.2%以下、W:3.0%以下、B:0.01%以下のうちから選ばれた1種または2種以上、
D群:Ca:0.01%以下、REM:0.01%以下のうちから選ばれた1種または2種
のうちから選ばれた1群または2群以上を含有することができる。
The above-mentioned components are basic components. In addition to the basic components, the following group A to group D: Group A: Al: 0.002 to 0.050%,
Group B: Cu: 3.5% or less,
Group C: Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less, W: 3.0% or less, B: 0.01% or less selected from 0.01% or less,
Group D: Ca: 0.01% or less, REM: One or more groups selected from one or two selected from 0.01% or less can be contained.

A群:Al:0.002〜0.050%、
A群:Alは、脱酸剤として作用する元素であり、このような効果を得るためには、0.002%以上含有することが好ましいが、0.050%を超えて含有すると、靭性に悪影響を及ぼす。このため、含有する場合には、A群:Al:0.002〜0.050%に限定することが好ましい。より好ましくは0.03%以下である。Al無添加の場合には、不可避的不純物としてAl:0.002%未満程度が許容される。
Group A: Al: 0.002 to 0.050%,
Group A: Al is an element that acts as a deoxidizer. In order to obtain such an effect, it is preferably contained in an amount of 0.002% or more, but if it exceeds 0.050%, the toughness is adversely affected. For this reason, when it contains, it is preferable to limit to A group: Al: 0.002-0.050%. More preferably, it is 0.03% or less. In the case where Al is not added, Al: less than 0.002% is allowed as an inevitable impurity.

B群:Cu:3.5%以下
B群:Cuは、保護皮膜を強固し、鋼中への水素の侵入を抑制し、耐硫化物応力腐食割れ性を高める。このような効果を得るためには0.5%以上含有することが望ましい一方、3.5%を超える含有は、CuSの粒界析出を招き、熱間加工性が低下する。このため、含有する場合には、B群:Cuは3.5%以下に限定することが好ましい。なお、より好ましくは0.8〜2.5%である。
Group B: Cu: 3.5% or less Group B: Cu strengthens the protective film, suppresses the penetration of hydrogen into the steel, and improves the resistance to sulfide stress corrosion cracking. In order to obtain such an effect, it is desirable to contain 0.5% or more, while the content exceeding 3.5% leads to precipitation of CuS grain boundaries and decreases hot workability. For this reason, when it contains, it is preferable to limit B group: Cu to 3.5% or less. In addition, More preferably, it is 0.8 to 2.5%.

C群:Nb:0.2%以下、Ti:0.3%以下、Zr:0.2%以下、W:3.0%以下、B:0.01%以下のうちから選ばれた1種または2種以上
C群:Nb、Ti、Zr、W、Bはいずれも、強度を増加させる元素であり、必要に応じて選択して含有できる。このような効果は、Nb:0.03%以上、Ti:0.03%以上、Zr:0.03%以上、W:0.2%以上、B:0.0005%以上の含有で認められる。一方、Nb:0.2%、Ti:0.3%、Zr:0.2%、W:3.0%、B:0.01%、をそれぞれ超える含有は、靭性を低下させる。このため、含有する場合は、Nb:0.2%以下、Ti:0.3%以下、Zr:0.2%以下、W:3.0%以下、B:0.01%以下に、それぞれ限定することが好ましい。
Group C: Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less, W: 3.0% or less, B: 0.01% or less selected from Group C: Nb, Ti , Zr, W, and B are elements that increase the strength, and can be selected and contained as necessary. Such effects are recognized when Nb: 0.03% or more, Ti: 0.03% or more, Zr: 0.03% or more, W: 0.2% or more, B: 0.0005% or more. On the other hand, inclusions exceeding Nb: 0.2%, Ti: 0.3%, Zr: 0.2%, W: 3.0%, and B: 0.01% respectively reduce toughness. For this reason, when it contains, it is preferable to limit to Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less, W: 3.0% or less, B: 0.01% or less, respectively.

D群:Ca:0.01%以下、REM:0.01%以下のうちから選ばれた1種または2種
D群:Ca、REMは、硫化物系介在物の形態を球状化する作用を有し、介在物周囲のマトリックスの格子歪を小さくして、介在物の水素トラップ能を低下させる効果を有し、必要に応じ選択して1種または2種を含有できる。このような効果を得るためには、Ca:0.0005%以上、REM:0.001%以上含有することが望ましいが、Ca:0.01%、REM:0.01%を超えて含有すると、耐食性が低下する。このため、含有する場合には、Caは0.01%以下に、REMは0.01%以下に限定することが好ましい。
Group D: Ca: 0.01% or less, REM: One or two types selected from 0.01% or less Group D: Ca, REM has the effect of spheroidizing the form of sulfide inclusions, and intervenes It has the effect of reducing the lattice strain of the matrix around the object and reducing the hydrogen trapping ability of the inclusions, and it can contain one or two kinds as required. In order to obtain such an effect, it is desirable to contain Ca: 0.0005% or more and REM: 0.001% or more. However, if it contains more than Ca: 0.01% and REM: 0.01%, the corrosion resistance decreases. For this reason, when it contains, it is preferable to limit Ca to 0.01% or less and REM to 0.01% or less.

上記した成分以外の残部は、Feおよび不可避的不純物である。なお、不可避的不純物としてはP:0.03%以下、S:0.005%以下が許容できる。
上記した組成を有する鋼素材の製造方法はとくに限定する必要はない。転炉、電気炉等、常用の溶製炉を使用して、上記した組成の溶鋼を溶製し、連続鋳造法等の常用の鋳造方法で、鋳片(丸鋳片)としたものを鋼素材とすることが好ましい。なお、鋳片を熱間圧延して所定寸法の鋼片として鋼素材としてもよい。また、造塊−分塊圧延法で鋼片とし、鋼素材としてもなんら問題はない。
The balance other than the above components is Fe and inevitable impurities. Inevitable impurities include P: 0.03% or less and S: 0.005% or less.
The method for producing a steel material having the above composition need not be particularly limited. Using a conventional smelting furnace such as a converter or electric furnace, the molten steel having the composition described above is melted, and a slab (round slab) is obtained by a conventional casting method such as a continuous casting method. It is preferable to use a raw material. In addition, it is good also as a steel raw material as a steel slab of a predetermined dimension by hot-rolling a slab. Moreover, it is set as a steel slab by the ingot-making-slab rolling method, and there is no problem as a steel raw material.

まず、上記した組成を有する鋼素材を、加熱装置に装入して、加熱温度:600℃以上融点未満の範囲の温度に加熱する。
加熱温度:600℃以上融点未満
加熱温度が600℃未満では、組織が単相であり、変態を利用した組織の微細化が達成できない。一方、融点以上では加工を施すことができない。このため、鋼素材の加熱温度は600℃以上融点未満の温度に限定した。なお、好ましくは変形抵抗が小さく加工が容易であり、冷却時の温度差を大きくとれるという観点から1000〜1300℃である。より好ましくは1100〜1300℃である。
First, a steel material having the above-described composition is charged into a heating device and heated to a temperature in the range of heating temperature: 600 ° C. or higher and lower than the melting point.
Heating temperature: 600 ° C. or higher and lower than the melting point When the heating temperature is lower than 600 ° C., the structure is a single phase, and the structure cannot be refined using transformation. On the other hand, processing cannot be performed above the melting point. For this reason, the heating temperature of the steel material was limited to a temperature of 600 ° C. or higher and lower than the melting point. The temperature is preferably 1000 to 1300 ° C. from the viewpoint that the deformation resistance is small and the processing is easy and the temperature difference during cooling can be increased. More preferably, it is 1100-1300 degreeC.

加熱された鋼素材は、ついで、穿孔圧延装置で穿孔圧延を施されて中空素材とされる。
穿孔圧延条件は、鋼素材を所定の中空素材とすることができれば、とくにその条件を限定する必要はなく、常用の穿孔圧延とすることが好ましい。
ついで、得られた中空素材は、冷却装置で冷却される。
冷却は、冷却開始温度からの温度差が少なくとも50℃以上で、かつ600℃以上となる冷却停止温度まで、中空素材の外表面位置の温度で1.0℃/s以上の平均冷却速度で冷却する加速冷却処理とする。なお、冷却開始温度とは、冷却開始前の中空素材の肉厚中心温度であり、本発明では600℃以上とすることが好ましい。冷却開始温度が600℃未満では、その後の加工による組織微細効果が期待できない。
The heated steel material is then subjected to piercing and rolling with a piercing and rolling device to form a hollow material.
The piercing and rolling conditions are not particularly limited as long as the steel material can be a predetermined hollow material, and it is preferable to use the usual piercing and rolling.
Next, the obtained hollow material is cooled by a cooling device.
Cooling is accelerated by cooling at an average cooling rate of 1.0 ° C / s or higher at the temperature of the outer surface position of the hollow material to a cooling stop temperature at which the temperature difference from the cooling start temperature is at least 50 ° C and 600 ° C or higher. Let it be a cooling process. The cooling start temperature is the thickness center temperature of the hollow material before the start of cooling, and is preferably 600 ° C. or higher in the present invention. When the cooling start temperature is less than 600 ° C., the fine structure effect by the subsequent processing cannot be expected.

冷却温度範囲:50℃以上
冷却の温度範囲、すなわち、冷却開始温度と冷却停止温度の温度差は、少なくとも表面温度で50℃以上とする。冷却の温度範囲が50℃未満では、顕著な非平衡状態の相分率を確保できなくなり、その後の加工により所望の組織微細化を達成できない。このため、冷却の温度範囲は50℃以上に限定した。冷却の温度範囲は大きいほど、非平衡状態の相分率を確保できやすくなる。なお、好ましくは100℃以上である。
Cooling temperature range: 50 ° C. or more The cooling temperature range, that is, the temperature difference between the cooling start temperature and the cooling stop temperature is at least 50 ° C. at the surface temperature. When the cooling temperature range is less than 50 ° C., it becomes impossible to secure a remarkable non-equilibrium phase fraction, and the desired structure refinement cannot be achieved by subsequent processing. For this reason, the temperature range of cooling was limited to 50 ° C. or higher. The larger the cooling temperature range, the easier it is to secure a non-equilibrium phase fraction. In addition, Preferably it is 100 degreeC or more.

冷却停止温度:600℃以上
冷却停止温度は600℃以上とする。冷却停止温度が600℃未満では、元素の拡散が遅くなり、その後の加工による相変態(α→γ変態)が遅れ、所望の加工による組織微細効果が期待できなくなる。このため、冷却停止温度は600℃以上に限定した。なお、好ましくは700℃以上である。なお、冷却停止時の温度が600℃未満でも、複熱やその後に加えられる熱間加工による加工発熱で600℃以上となる場合には、組織の微細化効果を発揮する。
Cooling stop temperature: 600 ° C or higher Cooling stop temperature shall be 600 ° C or higher. When the cooling stop temperature is less than 600 ° C., the diffusion of elements is delayed, the phase transformation (α → γ transformation) by the subsequent processing is delayed, and the microstructure effect by the desired processing cannot be expected. For this reason, the cooling stop temperature was limited to 600 ° C. or higher. In addition, Preferably it is 700 degreeC or more. Even if the temperature at the time of cooling stop is less than 600 ° C., the effect of refining the structure is exhibited when the heat generation due to double heat or subsequent hot processing is 600 ° C. or higher.

平均冷却速度:1.0℃/s以上
冷却の平均冷却速度が0.3℃/s未満では、非平衡状態の相分率を確保できなくなり、その後の加工により所望の組織微細化を達成できない。このため、冷却の平冷却速度は1.0℃/s以上に限定した。なお、冷却速度の上限は、冷却装置の能力により決定され、とくに限定する必要はないが、熱応力による割れ、曲がり防止の観点から、30℃/s以下とすることが好ましい。なお、より好ましくは3〜10℃/sである。
Average cooling rate: 1.0 ° C./s or more If the average cooling rate of cooling is less than 0.3 ° C./s, it is impossible to secure a phase fraction in a non-equilibrium state, and a desired microstructure cannot be achieved by subsequent processing. For this reason, the cooling rate of cooling is limited to 1.0 ° C./s or more. The upper limit of the cooling rate is determined by the capacity of the cooling device and is not particularly limited, but is preferably 30 ° C./s or less from the viewpoint of preventing cracking and bending due to thermal stress. More preferably, it is 3 to 10 ° C./s.

冷却を施された中空素材は、圧延装置で加工を施され、所定寸法の継目無鋼管とされる。なお、加工を施すまでの時間は冷却終了後600s以内とすることが好ましい。冷却終了後、加工開始までの時間が600sを超えて長くなると、フェライト相がオーステナイト相に変態し、非平衡状態を確保できにくくなる。
なお、加工後の冷却速度は、とくに限定する必要はないが、肉厚中心温度で平均冷却速度で20℃/sを超える冷却となる場合には、圧延装置の出側に配設された保温装置に装入し、平均冷却速度を20℃/s以下に調整することが好ましい。加工後の冷却が20℃/sを超えて速くなりすぎると、α→γ変態によるオーステナイト相の析出が遅れ、オーステナイト相を析出することなく冷却され、加工後の組織が凍結され、所望の組織微細化を達成することができなくなる。
The cooled hollow material is processed by a rolling device to be a seamless steel pipe having a predetermined size. In addition, it is preferable that the time until the processing is performed is within 600 s after the cooling is completed. If the time from the end of cooling to the start of processing exceeds 600 s, the ferrite phase transforms into an austenite phase, making it difficult to ensure a non-equilibrium state.
The cooling rate after processing is not particularly limited. However, when cooling is performed at an average cooling rate exceeding 20 ° C./s at the wall thickness center temperature, the heat retaining temperature provided on the outlet side of the rolling apparatus. It is preferable to charge the apparatus and adjust the average cooling rate to 20 ° C./s or less. If the cooling after processing exceeds 20 ° C / s and becomes too fast, the precipitation of the austenite phase due to the α → γ transformation is delayed, the austenite phase is cooled without precipitation, the processed structure is frozen, and the desired structure It becomes impossible to achieve miniaturization.

以上、冷却装置を、穿孔圧延装置と圧延装置の間に配設した装置列を使用した場合について説明した。本発明では、冷却装置を、加熱装置と穿孔圧延装置の間に配設した装置列を使用しても、同様の効果が期待できる。というのは、本発明では、穿孔圧延、あるいは圧延のいずれにおいても効果があり、加工装置の加工形態の影響は少ないことを確認している。   In the above, the case where the cooling apparatus used the apparatus row | line | column arrange | positioned between the piercing-rolling apparatus and the rolling apparatus was demonstrated. In the present invention, the same effect can be expected even when a cooling device using a device row arranged between a heating device and a piercing and rolling device is used. This is because, in the present invention, it is confirmed that there is an effect in both piercing and rolling, and the influence of the processing form of the processing apparatus is small.

冷却装置を加熱装置と穿孔圧延装置の間に配設した装置列を使用する場合には、冷却を行う温度範囲は、穿孔圧延が可能な温度以上となるように、鋼種に応じて冷却停止温度を設定する必要がある。本発明で使用する鋼素材の組成範囲であれば、冷却停止温度は、1000℃以上とすることが好ましい。冷却停止温度が600℃未満では、変形抵抗が高くなりすぎて穿孔圧延が困難となる。このため、この場合には、冷却停止温度は600℃以上に限定することが好ましい。また、加熱された鋼素材を冷却するに際し、非平衡状態の相分率を確保するためには、外表面位置での冷却速度で、平均で、1.0℃/s以上の冷却速度とすることが好ましい。   When using a device array in which the cooling device is arranged between the heating device and the piercing and rolling device, the cooling stop temperature is set according to the steel type so that the temperature range for cooling is equal to or higher than the temperature at which piercing and rolling can be performed. Need to be set. If it is the composition range of the steel raw material used by this invention, it is preferable that a cooling stop temperature shall be 1000 degreeC or more. When the cooling stop temperature is less than 600 ° C., the deformation resistance becomes too high and piercing and rolling becomes difficult. For this reason, in this case, the cooling stop temperature is preferably limited to 600 ° C. or higher. Further, when cooling the heated steel material, in order to ensure a non-equilibrium phase fraction, the cooling rate at the outer surface position should be, on average, a cooling rate of 1.0 ° C./s or more. preferable.

上記した製造方法で得られる継目無鋼管は、上記した組成と、マルテンサイト相を主相とし、フェライト相と、あるいはさらに残留オーステナイト相からなる組織とを有する鋼管である。ここでいう「主相」とは、もっとも多い相をいうものとする。なお、残留オーステナイト相は、面積率で20%以下とすることが好ましい。このような組織を有する鋼管は、降伏強さ:654MPa超えの高強度と、肉厚中心位置でのシャルピー衝撃試験の試験温度:−40℃での吸収エネルギーが50J以上となる優れた低温靭性と、炭酸ガスを含み、230℃という高温で苛酷な腐食環境下における耐食性に優れた鋼管となる。 The seamless steel pipe obtained by the above-described manufacturing method is a steel pipe having the above-described composition and a structure including a martensite phase as a main phase, a ferrite phase, and a residual austenite phase. The “main phase” here refers to the most common phase. The residual austenite phase is preferably 20% or less in terms of area ratio. A steel pipe having such a structure has a high strength exceeding yield strength: 654 MPa, an excellent low temperature toughness with an absorbed energy at a Charpy impact test at the center of the wall thickness of −40 ° C. of 50 J or more. It contains carbon dioxide and becomes a steel pipe with excellent corrosion resistance in a severe corrosive environment at a high temperature of 230 ° C.

つぎに、実施例に基づき、さらに本発明について説明する。   Next, the present invention will be further described based on examples.

表1に示す組成の鋼素材を出発素材とした。これら鋼素材は、転炉で溶製した溶鋼を、連続鋳造法で鋳片とし、該鋳片を成型圧延で表1に示す組成の丸鋼片(230mmφ)としたものである。これら鋼素材を用いて厚肉継目無鋼管(外径273mmφ×肉厚32mm)とした。
これら鋼素材を、図1(a)に示す装置列の加熱装置1に装入し、表2に示す加熱温度に加熱し一定時間(60min)保持したのち、バレル形ロールのマンネスマン式穿孔圧延装置2を用いて穿孔圧延を施して中空素材(肉厚:約50mm)とし、スプレーによる冷却水を冷媒とする冷却装置4で、表2に示す平均冷却速度で、表2に示す冷却停止温度まで冷却し、直ちにエロンゲータ、プラグミル、リーラ、サイザーを順次配列してなる圧延装置3で表2に示す累積圧下率で圧延し、継目無鋼管(外径273mmφ×肉厚25〜50mm)とした。なお、圧延後は放冷(0.1〜1.5℃/s)した。得られた厚肉継目無鋼管にさらに熱処理(焼入焼戻処理あるいは焼戻処理)を施した。
A steel material having the composition shown in Table 1 was used as a starting material. In these steel materials, molten steel melted in a converter is made into a slab by a continuous casting method, and the slab is made into a round steel piece (230 mmφ) having a composition shown in Table 1 by forming and rolling. These steel materials were used to make thick-walled seamless steel pipes (outer diameter 273 mmφ x wall thickness 32 mm).
These steel materials are charged into the heating device 1 of the apparatus row shown in FIG. 1 (a), heated to the heating temperature shown in Table 2 and held for a certain time (60min), and then a Mannesmann piercing and rolling apparatus with a barrel roll. 2 is used for piercing and rolling to form a hollow material (thickness: about 50 mm), and using a cooling device 4 that uses cooling water by spraying as a refrigerant, at the average cooling rate shown in Table 2, up to the cooling stop temperature shown in Table 2 It was cooled and immediately rolled with a rolling reduction device 3 in which an elongator, a plug mill, a reeler, and a sizer were sequentially arranged at the cumulative reduction shown in Table 2 to obtain a seamless steel pipe (outer diameter 273 mmφ × thickness 25-50 mm). In addition, after rolling, it was allowed to cool (0.1 to 1.5 ° C./s). The resulting thick-walled seamless steel pipe was further subjected to heat treatment (quenching / tempering treatment or tempering treatment).

得られた厚肉継目無鋼管から、試験片を採取して組織観察、引張試験、衝撃試験を実施した。試験方法はつぎのとおりとした。
(1)組織観察
得られた鋼管から、組織観察用試験片を採取し、管長手方向に直交する断面(C断面)を研磨、腐食(腐食液:ビレラ液)して、光学顕微鏡(倍率:100倍)または走査型電子顕微鏡(倍率:1000倍)で組織を観察し、撮像して、画像解析を用い、組織の種類およびその分率を測定した。なお、組織写真から、単位長さの直線と交差する相境界の数を測定し、結晶粒のサイズ指標とし、微細化の指標とした。なお、単位長さ当たりの相境界数は、得られた値を、鋼管No.5の値を基準(1.00)として、基準値に対する比率として示した。
Test pieces were collected from the resulting thick-walled seamless steel pipe and subjected to structure observation, tensile test, and impact test. The test method was as follows.
(1) Microstructure observation A specimen for microstructural observation is collected from the obtained steel pipe, and a cross section (C cross section) perpendicular to the longitudinal direction of the pipe is polished and corroded (corrosive liquid: Villera liquid), and an optical microscope (magnification: 100 times) or a scanning electron microscope (magnification: 1000 times), the tissue was observed, imaged, and image analysis was used to measure the type and fraction of the tissue. Note that the number of phase boundaries intersecting with the unit length straight line was measured from the structure photograph, and used as a crystal grain size index and a refinement index. In addition, the number of phase boundaries per unit length was shown as a ratio to the reference value, with the obtained value being the value of steel pipe No. 5 as the reference (1.00).

(2)引張試験
得られた鋼管から、管軸方向が引張方向となるように、丸棒引張試験片(平行部6mmφ×G.L.20mm)を採取し、引張試験を実施し、降伏強さYS、引張強さTSを求めた。なお、降伏強さは0.2%伸びでの強度とした。
(3)衝撃試験
得られた鋼管の肉厚中央位置から、管軸方向が試験片長手方向となるように、Vノッチ試験片を採取し、JIS Z 2242の規定に準拠してシャルピー衝撃試験を実施し、試験温度:−40℃における吸収エネルギーを測定し、靭性を評価した。なお、試験片は各3本とし、それらの平均値を当該鋼管の吸収エネルギーとした。
(2) Tensile test From the obtained steel pipe, take a round bar tensile test piece (parallel part 6mmφ x GL20mm) so that the tube axis direction is the tensile direction, conduct a tensile test, yield strength YS, tensile We asked for strength TS. The yield strength was 0.2% elongation.
(3) Impact test V-notch test specimens are collected from the center position of the thickness of the obtained steel pipe so that the pipe axis direction is the longitudinal direction of the specimen, and Charpy impact tests are conducted in accordance with the provisions of JIS Z 2242. The test was carried out to measure the absorbed energy at a test temperature of −40 ° C. to evaluate toughness. The number of test pieces was three each, and the average value thereof was taken as the absorbed energy of the steel pipe.

得られた結果を、表3に示す。   The results obtained are shown in Table 3.

Figure 0006171851
Figure 0006171851

Figure 0006171851
Figure 0006171851

Figure 0006171851
Figure 0006171851

本発明例はいずれも、厚肉の肉厚中心位置においても組織の微細化ができ、降伏強さ:654MPa超えの高強度であるにもかかわらず、シャルピー衝撃試験の試験温度:−40℃における吸収エネルギーが50J以上と靭性が顕著に向上している。なお、加工量(圧下率)が0%と低い本発明例(鋼管No.11)でも、靭性が顕著に向上している。一方、本発明の範囲を外れる比較例は、所望の高強度を確保できていないか、組織が微細化できず、所望の高靭性を確保できていない。 In all of the examples of the present invention, the structure can be refined even at the thickness center position of the thick wall, and although the yield strength is higher than 654 MPa, the Charpy impact test temperature is −40 ° C. Absorbed energy is 50J or more, and the toughness is remarkably improved. In addition, the toughness is remarkably improved even in the present invention example (steel pipe No. 11) having a low processing amount (rolling rate) of 0%. On the other hand, the comparative example which is out of the scope of the present invention does not ensure the desired high strength, or the structure cannot be refined, and the desired high toughness cannot be ensured.

1 加熱装置
2 穿孔圧延装置
3 圧延装置
4 冷却装置
31 エロンゲータ
32 プラグミル
33 サイジングミル(サイザー)
1 Heating device 2 Punching and rolling device 3 Rolling device 4 Cooling device
31 Elongator
32 Plug mill
33 Sizing mill (sizer)

Claims (5)

鋼素材を加熱する加熱装置と、該加熱された鋼素材に穿孔圧延を施し中空素材とする穿孔圧延装置と、該中空素材に加工を施し所定形状の継目無鋼管とする圧延装置とをこの順に配設してなる継目無鋼管製造用装置列において、前記鋼素材が、マルテンサイト系ステンレス鋼組成を有する鋼素材であり、前記加熱装置が、前記鋼素材を加熱温度:600℃以上融点未満に加熱することができる加熱能を有する加熱装置であり、前記加熱装置と前記穿孔圧延装置との間で該加熱装置の出側でかつ該穿孔圧延装置の入側に、または前記穿孔圧延装置と前記圧延装置との間で該穿孔圧延装置の出側でかつ該圧延装置の入側に、冷却開始温度からの温度差が少なくとも50℃以上でかつ600℃以上となる冷却停止温度までの温度域を、被冷却材の外表面位置の平均冷却速度で1.0℃/s以上が得られる冷却能を有し、被冷却材の組織を非平衡状態の組織とすることができる冷却装置を配設してなることを特徴とする厚肉ステンレス継目無鋼管製造用装置列。 A heating device for heating a steel material, a piercing and rolling device for subjecting the heated steel material to piercing and rolling to form a hollow material, and a rolling device for processing the hollow material to obtain a seamless steel pipe having a predetermined shape in this order. In the apparatus row for seamless steel pipe production, the steel material is a steel material having a martensitic stainless steel composition, and the heating device heats the steel material to a heating temperature of 600 ° C. or higher and lower than the melting point. A heating device having a heating capability capable of being heated, and between the heating device and the piercing and rolling device, on the exit side of the heating device and on the entry side of the piercing and rolling device, or the piercing and rolling device and the A temperature range from the cooling start temperature to the cooling stop temperature at which the temperature difference from the cooling start temperature is at least 50 ° C. or more and 600 ° C. or more is provided between the rolling device and the exit side of the piercing and rolling device and on the entry side of the rolling device. , of the outer surface position of the coolant Thick, characterized in that have a cooling ability 1.0 ° C. / s or more average cooling rate is obtained, formed by disposing can be Ru cooler be organized in a non-equilibrium state tissue of a coolant Equipment line for stainless steel seamless steel pipe manufacturing. 前記圧延装置の出側に、保温装置を配設することを特徴とする請求項1に記載の厚肉ステンレス継目無鋼管製造用装置列。   The apparatus for manufacturing a thick-walled stainless steel seamless steel pipe according to claim 1, wherein a heat retaining device is disposed on the outlet side of the rolling device. 請求項1または2に記載の厚肉ステンレス継目無鋼管製造用装置列を利用した厚肉ステンレス継目無鋼管の製造方法であって、鋼素材を前記加熱装置で加熱後、前記穿孔圧延装置で穿孔圧延を施して中空素材とし、さらに該中空素材を前記冷却装置で冷却したのち、前記圧延装置で加工を施して、あるいはさらに該加工後に前記保温装置を通過させる処理を施して、さらに焼入焼戻処理あるいは焼戻処理からなる熱処理を施し、所定寸法の厚肉ステンレス継目無鋼管とするにあたり、
前記鋼素材を、質量%で、
C:0.050%以下、 Si:0.50%以下、
Mn:0.20〜1.80%、 Cr:15.5〜18.0%、
Ni:1.5〜5.0%、 Mo:1.0〜3.5%、
V:0.02〜0.20%、 N :0.01〜0.15%、
O:0.006%以下
を含み、残部Feおよび不可避的不純物からなる組成を有する鋼素材とし、
前記加熱を、600℃以上融点未満の温度に加熱する処理とし、前記穿孔圧延を施したのちで、前記冷却装置で冷却する前の前記中空素材の表面温度を冷却開始温度として、前記冷却を、表面温度で、前記冷却開始温度からの温度差が少なくとも50℃以上で、かつ600℃以上となる冷却停止温度まで、外表面温度で1.0℃/s以上の平均冷却速度で冷却する処理とし、前記厚肉ステンレス継目無鋼管が、管軸方向の降伏強さが654MPa超えの高強度と、肉厚中心部でシャルピー衝撃試験の試験温度:−40℃での管軸方向における吸収エネルギーが50J以上となる優れた低温靭性とを兼備する高強度厚肉ステンレス継目無鋼管である
ことを特徴とする低温靭性に優れた油井用高強度厚肉ステンレス継目無鋼管の製造方法。
A method for producing a thick stainless steel seamless steel pipe using the apparatus for producing a thick stainless steel seamless steel pipe according to claim 1 or 2, wherein a steel material is heated by the heating device and then punched by the piercing and rolling device. A hollow material is formed by rolling, and the hollow material is further cooled by the cooling device, then processed by the rolling device, or further processed by passing through the heat retaining device after the processing, and further quenched and hardened. When performing heat treatment consisting of tempering treatment or tempering treatment to make a thick stainless steel seamless steel pipe of a predetermined size,
The steel material in mass%,
C: 0.050% or less, Si: 0.50% or less,
Mn: 0.20-1.80%, Cr: 15.5-18.0%,
Ni: 1.5-5.0%, Mo: 1.0-3.5%,
V: 0.02 to 0.20%, N: 0.01 to 0.15%,
O: A steel material containing 0.006% or less and having the balance Fe and inevitable impurities,
The heating is performed at a temperature of 600 ° C. or higher and lower than the melting point, and after the piercing and rolling, the surface temperature of the hollow material before cooling with the cooling device is set as a cooling start temperature, and the cooling is performed. At the surface temperature, the temperature difference from the cooling start temperature is at least 50 ° C. or more, and the cooling is performed at an outer surface temperature at an average cooling rate of 1.0 ° C./s or more to a cooling stop temperature that is 600 ° C. or more. Thick-walled stainless steel seamless pipe has a high strength with a yield strength exceeding 654 MPa in the tube axis direction, and a Charpy impact test temperature at the center of the wall thickness: Absorbed energy in the tube axis direction at -40 ° C is 50 J or more. A method for producing a high-strength, thick stainless steel seamless steel pipe for oil wells having excellent low-temperature toughness, characterized by being a high-strength, thick-walled stainless steel seamless steel pipe having both excellent low-temperature toughness.
前記加工後に前記保温装置内を通過させる処理が、平均冷却速度で20℃/s以下の冷却となるように調整する処理とすることを特徴とする請求項3に記載の油井用高強度厚肉ステンレス継目無鋼管の製造方法。   The high-strength thick wall for oil wells according to claim 3, wherein the process of passing through the heat retaining device after the processing is adjusted so that the average cooling rate is 20 ° C / s or less. Manufacturing method of stainless steel seamless steel pipe. 前記組成に加えてさらに、質量%で、下記A群〜D群のうちから選ばれた1群または2群以上を含有することを特徴とする請求項3または4に記載の油井用高強度厚肉ステンレス継目無鋼管の製造方法。

A群:Al:0.002〜0.050%、
B群:Cu:3.5%以下、
C群:Nb:0.2%以下、Ti:0.3%以下、Zr:0.2%以下、W:3.0%以下、B:0.01%以下のうちから選ばれた1種または2種以上、
D群:Ca:0.01%以下、REM:0.01%以下のうちから選ばれた1種または2種
The high strength thickness for oil wells according to claim 3 or 4, further comprising one group or two or more groups selected from the following groups A to D in mass% in addition to the composition. Manufacturing method of meat stainless steel seamless steel pipe.
Group A: Al: 0.002 to 0.050%,
Group B: Cu: 3.5% or less,
Group C: Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less, W: 3.0% or less, B: 0.01% or less selected from 0.01% or less,
Group D: Ca: 0.01% or less, REM: One or two selected from 0.01% or less
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016183404A (en) * 2015-03-25 2016-10-20 Jfeスチール株式会社 Method for producing dual phase stainless seamless steel tube

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3225318B1 (en) 2014-11-27 2024-08-21 JFE Steel Corporation Manufacturing method for duplex stainless steel seamless pipe or tube using a device array for manufacturing seamless steel pipe or tube
US10876183B2 (en) 2015-07-10 2020-12-29 Jfe Steel Corporation High-strength seamless stainless steel pipe and method of manufacturing high-strength seamless stainless steel pipe
US20180204423A1 (en) * 2015-12-25 2018-07-19 Hitachi-Omron Terminal Solutions, Corp. Automatic transaction system
CN106064183A (en) * 2016-07-18 2016-11-02 内蒙古北方重工业集团有限公司 A kind of slow cooling method containing Cr, Mo alloy large-size extruding heavy wall steps of manufacturing blanks
CA3026554C (en) * 2016-07-27 2021-03-23 Jfe Steel Corporation High-strength seamless stainless steel pipe for oil country tubular goods, and method for producing the same
CN109158422A (en) * 2018-08-06 2019-01-08 宁波大学 A kind of forming device for high-speed rail hole-bored axle from end to end
CN110756616B (en) * 2019-10-30 2021-04-30 江苏隆达超合金股份有限公司 Preparation method for reducing high-carbon martensitic stainless steel pipe
CN113913708A (en) * 2021-09-08 2022-01-11 邯郸新兴特种管材有限公司 95-steel-grade super 13Cr seamless steel pipe and production method thereof

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52152814A (en) * 1976-06-14 1977-12-19 Nippon Steel Corp Thermo-mechanical treatment of seamless steel pipe
JPS57100806A (en) * 1980-12-16 1982-06-23 Nippon Kokan Kk <Nkk> Producing device for seamless steel pipe
JPS57127505A (en) * 1981-01-22 1982-08-07 Nippon Steel Corp Direct rolling manufacturing device for steel
JPH05195059A (en) * 1992-01-13 1993-08-03 Nippon Steel Corp Production of thick steel plate having fine metallic structure
JPH101755A (en) 1996-04-15 1998-01-06 Nippon Steel Corp Martensitic stainless steel excellent in corrosion resistance and sulfide stress corrosion cracking resistance and its production
DE60231279D1 (en) 2001-08-29 2009-04-09 Jfe Steel Corp Method for producing seamless tubes of high-strength, high-strength, martensitic stainless steel
JP3937964B2 (en) * 2001-08-29 2007-06-27 Jfeスチール株式会社 High strength and high toughness martensitic stainless steel seamless pipe manufacturing method
JP2003105441A (en) * 2001-09-28 2003-04-09 Kawasaki Steel Corp METHOD FOR MANUFACTURING SEAMLESS TUBE OF 13 Cr MARTENSITIC STAINLESS STEEL HAVING HIGH STRENGTH AND HIGH TOUGHNESS
PL203879B1 (en) 2002-01-09 2009-11-30 Sms Meer Gmbh Method and rolling stand for producing rods, bar stock or seamless tubes
JP2004124188A (en) * 2002-10-03 2004-04-22 Mitsubishi Heavy Ind Ltd HIGH Cr HEAT-RESISTANT STEEL AND METHOD FOR MANUFACTURING THE SAME
JP5109222B2 (en) 2003-08-19 2012-12-26 Jfeスチール株式会社 High strength stainless steel seamless steel pipe for oil well with excellent corrosion resistance and method for producing the same
CN100451153C (en) 2003-08-19 2009-01-14 杰富意钢铁株式会社 High strength stainless steel pipe excellent in corrosion resistance for use in oil well and method for production thereof
RU2336133C1 (en) * 2004-07-20 2008-10-20 Сумитомо Метал Индастриз, Лтд. Method of chrome-containing steel hot working
WO2006088107A1 (en) * 2005-02-16 2006-08-24 Sumitomo Metal Industries, Ltd. Process for producing seamless steel pipe
DE102010008389A1 (en) * 2010-02-17 2011-08-18 Kocks Technik GmbH & Co. KG, 40721 Rolling system for producing seamless metallic pipe, has induction system provided between front rolling device and rear rolling device for influencing temperature of intermediate product before product is supplied to rear rolling device
BR112012026595A2 (en) * 2010-04-19 2016-07-12 Jfe Steel Corp CR-containing steel pipe for pipe for excellent conduction in resistance to crevice corrosion cracking in heat-affected welded zone
DE102010052084B3 (en) * 2010-11-16 2012-02-16 V&M Deutschland Gmbh Process for the economic production of seamless hot-rolled tubes in continuous tube rolling mills
JP5273231B2 (en) * 2011-11-01 2013-08-28 新日鐵住金株式会社 Manufacturing method of seamless metal pipe

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016183404A (en) * 2015-03-25 2016-10-20 Jfeスチール株式会社 Method for producing dual phase stainless seamless steel tube

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